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Economics of acetic acid production by partial oxidation of ethane

Article  in  APCBEE Procedia · December 2012

DOI: 10.1016/j.apcbee.2012.06.070

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APCBEE Procedia 3 (2012) 200 – 208

ICCCP 2012: 5-6 May 2012, Kuala Lumpur, Malaysia

Economics of Acetic Acid Production by Partial Oxidation of

Ethane
Moustafa Soliman a*, Yousef Al-Zeghayera,b, Abdulrhman S.Al-Awadia, Sulaiman
Al-Maymanc
a
Department of Chemical Engineering, College of Engineering, King Saud University, P.O. Box 800, Riyadh 11421, Saudi Arabia
b
Director of Industrial Catalysts Chair
c
Energy Research Institute, KACST, Riyadh, Saudi Arabia

Abstract

Catalysts based on Mo, V, Nb mixed oxides can effect the partial oxidation of ethane to acetic acid . The process requires
a pressure of about 20 atm and acetic acid selectivity is about 20%, while ethylene selectivity is about 70%. The addition
of Pd to the MoVNb catalyst greatly increases the selectivity to acetic acid to about 80% and completely oxidizes CO to
CO2. In this paper, the economics of acetic acid production by partial oxidation of ethane will be evaluated and compared
with the carbonylation of methanol. In particular we study operating fixed bed reactors in series and in two steps. In the
first step ethylene is produced and co-produced water is separated. In the second step ethylene is oxidized to acetic acid.
This mode of operation increases the concentration of acetic acid leading to great saving in the product cost.

© 2012
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Open access under CC BY-NC-ND license.

Keywords acid: Economics , Ethane, Ethylene, Acetic Acid, Partial oxidation

1. Introduction

Commercially, acetic acid is mainly produced from methanol carbonylation which gives rise to many
problems, such as corrosion and waste disposal. Methanol carbonylation accounts for 65% of the world
capacity. Other processes for acetic acid production include oxidation of acetaldehyde , oxidation of naphtha

* Corresponding author
E-mail address: mostf34@hotmail.com

2212-6708© 2012 Published by Elsevier B.V. Selection and/or peer review under responsibility of Asia-Pacific Chemical,
Biological & Environmental Engineering Society Open access under CC BY-NC-ND license.
doi:10.1016/j.apcbee.2012.06.070
 Moustafa Soliman et al. / APCBEE Procedia 3 (2012) 200 – 208 201

and n-butane and fermentation of hydrocarbons. It is also produced as by-product in the manufacture of
cellulose acetate and polyvinyl alcohol. Showa Denko of Japan patented a one-step direct oxidation of
ethylene into acetic acid using a palladium-based heteropoly acids catalyst. A 100 KT/year plant based on this
patent is working now. In Saudi Arabia, ARAMCO sells methane and ethane to local manufacturers at the
low price of $0.75/million Btu. This makes the idea of direct oxidation of ethane to acetic acid very attractive.
In 2005, SABIC of Saudi Arabia commercialized a 30,000 tonnes/year acetic acid plant based on a proprietary
catalytic oxidation process. The catalyst is a calcined mixture of oxides of Mo, V, Nb and Pd, allows
selectivities to acetic acid as high as 80%. Combining this technology with low cost ethane may result in
production economics competitive with methanol carbonylation technology.The main exothermic reaction
equations describing the oxidation of ethane are

C2H6 + 1/2 O2 Æ C2H4 + H2O ΔH 600 0K = - 24.59 kcal/mole C2H4

C2H6 + 3/2 O2 Æ CH3COOH + H2O ΔH 600 0K = - 116.54 kcal/mole CH3COOH
C2H6 + 5/2 O2 Æ 2CO + 3H2O ΔH 600 0K = - 90.13 kcal / mole CO
C2H6 + 7/2 O2 Æ 2CO2 + 3H2O ΔH 600 0K = -157.92 Kcal / mole CO2
The study of MoVNb catalyst for the partial oxidation of ethane to ethylene and acetic acid was pioneered
by the work of Thorsteinson et al. [1] and Young and Thorsteinson [2]. The use of high pressure improves the
selectivity to acetic acid. The process requires a pressure of about 20 atm and acetic acid selectivity is about
20%, while ethylene selectivity is about 70%. Three patents by Karim et al.[3-5] have been granted to SABIC
as a result of work carried out at King Saud University. In these patents, it is shown that the addition of Pd to
the MoVNb catalyst greatly increases the selectivity to acetic acid to about 80% and completely oxidizes CO
to CO2. The same idea was also discovered by Borchert and Dingerdissen [6].The mechanism and the kinetics
of the reaction for MoV0.25Nb0.12Pd0.0005Ox catalyst were presented by Linke et al. [7,8].Kinetic expressions
for MoVNb catalyst with different compositions are given by Thorsteinson et al [1] and Rahman et al. [9].
Smejkal et al. [10] have analyzed the process of acetic acid manufacture using the MoVNb Pd catalyst and
made a comparison between acetic acid production cost by ethane oxidation and methanol carbonylation
giving 14% more production cost for the ethane oxidation scheme. With the possibility of continuous catalyst,
and reactor design improvements and process design optimization, this difference may be eliminated. On the
catalyst improvement side,Ellis [11] found that gold and another elements such as Sn, Ag, Cu, Fe or Sb can
replace Pd to increase the selectivity to acetic acid. Brazdil et al. [12] showed that the addition of Sn and Ti to
the standard MoVNb catalyst could be used to control ethylene to acetic acid ratio with Ti favoring acetic acid
formation. Bergh et al [13] found that Ni, Sb, and Ce could replace Nb. Ryan [14] replaced Nb with Ta & Te.
He found that the catalyst has high ethane conversion and ethylene selectivity with very low selectivity to
carbon oxides. For oxydehydrogenation reactors design ,the main concern in is to minimize oxygen
concentration in contact with the hydrocarbon to avoid undesired combustion reactions. Several ideas have
been explored including Staged Feed of Oxygen (multiple injection points) (Al-Sherehy et al [15]) ,
Membrane Reactors (Tonkovich et al. [16]) , Fluidized Bed Reactors (Zeyss et al.[17],cook et al.[18]),
Fluidized Bed Membrane Reactors (FLBMR)(Ahchieva et al. [19]), Electrochemical Reactors (Takeh ira et
al.[20]), Cycling Technology based on the redox nature of the catalyst (alternate feed of reactants)(Cavani et
al.[21]) and Microchannel Reactors (Brophy et al. [22]). For process design optimization, Rodriguez et al
[23] presented a systematic identification procedure .In this paper, we take on the partial oxidation process,
and study the economics of certain reactors arrangement.

2. The Partial Oxidation Process Description

A modified Union Carbide process [24] is shown in Fig. 1. Ethane and oxygen are mixed and fed to four
202 Moustafa Soliman et al. / APCBEE Procedia 3 (2012) 200 – 208

fixed bed reactors in series or a fluidized bed at a temperature of about 550 °K and pressure of 20 atm. The
reactors contain a catalyst of mixed oxides of Mo, V Nb and Pd supported on alumina. Oxygen mole fraction
in the feed should not exceed 0.06 to avoid the formation of a flammable mixture. This leads to a low ethane
conversion, and this in turn necessitates the use of more than one reactor in series in which fresh oxygen are
fed in each reactor. Water vapour favours the formation of acetic acid. Also high pressure and low
temperature favour acetic acid formation. The reaction heat is absorbed by pressurized water to generate
medium pressure saturated steam. The gaseous product from the last reactor is cooled down to condense part
of the acetic acid and water. The remaining acetic acid is removed in a flash chamber or a scrubber using
water. The condensed acetic acid and water is sent to an acetic acid concentration plant consisting of a
binary distillation column or an azeotropic distillation column which could use ethyl acetate as an entainer to
form an azeotrope with water. The uncondensed product consisting mainly of ethane and CO2 is recycled. In
the original Union carbide process, carbon dioxide is separated using, for example, an amine absorbing and
stripping system. Subsequent research indicated that recycling carbon dioxide is economically beneficial.

Fig. 1. Partial oxidation of ethane by total recycle (Four reactors).

The standard oil process (Wagner et al. [25])is based on a catalyst patented by British Petroleum (Kiston
[26]). The catalyst contains a mixed oxide of Mo, V, Nb, Re, Ca, Sb. It has the advantage that in presence of
steam vapour, acetic acid selectivity up to 78% can be obtained. Since ethylene CO, CO2 mole fractions in
the reactor effluent are relatively low, one can envisage a process in which the product gases are recycled to
the reactor after purging a small portion of that gas. If the reaction is carried out in a fluidized bed reactor,
one can feed the oxygen directly into the reactor where it is directly mixed and reacts with ethane. In this way
one can use a higher O2% than that can be used in a fixed bed reactor. This leads to higher ethane conversion.
Other advantages that can be gained from this process are as follows:
(i) The elimination of the CO2 separation system.
(ii) The elimination of the cryogenic separation section to separate ethylene.
(iii) The recycled carbon oxides serve as diluents to absorb the heat of reaction and avoid the
formation of flammable mixture.
(iv) The back mixing characteristics of fluidized bed helps increase the selectivity of acetic acid and
decrease the selectivity of ethylene.
 Moustafa Soliman et al. / APCBEE Procedia 3 (2012) 200 – 208 203

(v) The heat transfer coefficient in fluidized bed between the reactants and the coolant is much
higher in fluidized bed that in fixed bed reactors.
The main disadvantage of this process is that due to the back mixing characteristics of the fluidized bed,
we need a bigger reactor volume and thus more of the expensive catalyst than would be required in a fixed
bed. Also, because of the need to use water vapor in the reaction system to increase acetic acid selectivity, the
acetic acid concentration will be low requiring more expensive acetic acid concentration units.
The following modifications are recently suggested; McSwain and Seaman [27] suggested to treat the
effluent of ethane oxidation reactor in a predehydration tower so as to separately recover water, acetic acid,
and a gas stream for recycle back to the ethane oxidation reactor. The predehydration tower has 25-35
stages.Johnston et al [28] suggested an integrated, optimized process for the production of ethylene, carbon
monoxide and acetic acid from an ethane feed, including reacting ethane with oxygen in the presence of a
certain catalyst to produce ethylene, carbon monoxide and acetic acid in a reactor. Carbon monoxide can be
made use of in any other chemical reaction, e.g., producing acetic acid through carbonylation of methanol.
Ferguson et al. [29] found that if CO is introduced in the feed to the reactor, the amount of CO formed is
suppressed. The suppression of CO is not compensated by an equivalent increase in the CO2 formation,
resulting in a net decrease in total carbon oxides (COx) formation and an increase in acetic acid
selectivity.Ryan and Foster [30] suggested operating two reactors in series one at high temperature (about
450 C) and the other at low temperature ( about 200 C) to transform any ethylene from the first reactor to
acetic acid.

3. Process Economics

Fakeeha et al. [31] studied the process economics of the process with the following modifications on the
basic flow sheet ,use of air instead of oxygen,changing the inlet temperature of the reactants to the
reactor,increasing the number of fixed bed reactors to increase conversion and reduce recycle,and using a
fluidized bed reactor. They concluded that oxygen is preferred to air as oxidant. There is an optimum number
of reactors resulting from the trade off between increased conversion and increased capital cost. Th study
indicated that the number of fixed bed reactors in series with inter-oxygen injection should be four or more.
Smejkal et al. [10]concluded also that oxygen should be used as oxidant. They investigated the addition of
water vapor to the the reactants mix. Although the addition of water vapor increases selectivity to acetic acid,
the increased cost of separating acetic acid from water indicates that water vapor addition is not recommended.
Recycling of the unreacted reactants with CO2 is recommended. In fact in another paper Rodriguez et al. [23]
have shown that the use of a series of reactors with internal recycling reduces the cost of acetic acid
production. The use of a fluidized bed followed by a fixed bed reactor is an option that can be studied. The
fluidized bed is designed such that not all oxygen is consumed thus reducing catalyst volume. The oxygen
remaining is further reacted in the fixed bed. The process economics is studied for the case of acetic acid
production. Acetic Acid will be produced at the rate of about 136 Kt/year . In evaluating the economics of
the basic flow sheet and its modification the following data are used:
(1) Raw Material Costs: Ethane; 33$ /t (equivalent to 0.75 $ / MM Btu), Oxygen:
55$/t ,Catalyst;110 $/kg
(2) Utility Costs: Natural gas;0.75 $/MM Btu ,Electricity;3 c/Kwh, Cooling water (sea water); 30
c/ m3.,Process water;12$ / m3 .
The following assumptions are also made: Ethane and oxygen are supplied at 20 atm., Catalyst life is five
years, The location factor for Saudi Arabia is 1.25.and Stream factor is 0.9.
204 Moustafa Soliman et al. / APCBEE Procedia 3 (2012) 200 – 208

3.1. Equipment Design

For reactor design,the kinetics for the partial oxidation of ethane is based on the work of Thorsteinson et al.
[1] for MoVNb catalyst. The kinetics of acetic acid formation is multiplied by a factor to account for the
increased acetic acid selectivity due to the addition of Pd. Reactor simulation was carried out using the model
presented by Fakeeha et al [32] For reactors with ethane flow rate = 0.3 Kg mole/hr tube ,O2 : C2H2 = 6 : 94
and coolant temperature = inlet temperature = 550 °K, the following design parameters are obtained
Reactor tube length = 3.0 m,Reactor tube diameter = 0.0254 m,Number of tubes in a reactor = 12370 tubes
Reactor shell diameter = 4.8 m,Catalyst weight = 103 ton,,Ethane per pass conversion = 10.4%,Acetic acid
selectivity = 74.5%
For the scrubber;
Cooling and condensing the gas mixture to 44 °C, Scrubber Inlet Temperature = 44 °C,Scrubber Number
of Stages = 4,Acetic acid concentration to the concentration plant= 52% by weight
For acetic acid concentration, Brown [33] reached the conclusion that extraction to be the most favorable
approach except for feeds above 80% acetic acid, in which case azeotropic distillation becomes preferable.
From this study and that of Brown [33], we established the following formulae for the calculation of the acetic
acid concentration section purchased cost ( for 2011) and utilities.
Acetic Acid Concentration Plant Purchased Cost = 70* 106 / X0.7 $, X = Weight percent of acetic acid
Utilities:Electricity =50/X Kwt.h/1000 kg Acetic Acid
Steam = 60/X Kg/Kg Acetic Acid
Cooling Water = 2400/X Kg Water/ Kg Acetic AQcid

3.2. Cost Analysis:

Cost estimation using cost data from Peters et al.[34] updated using 2011 chemical engineering plant cost
index is given in table 1. In the first column we give cost analysis for the case of using one fluidized. Due to
backmixing, the catalyst weight is three times larger than the cases of 4 fixed bed reactors. This accounts for
higher product cost. In the second column we give cost analysis for the flow diagram shown in Figure 1 using
as catalyst MoVNbPd.

Table 1. Acetic acid cost calculations.

Number of Reactors 1 Fluid. Bed 4 Fixed Bed 4 Fixed Bed

Reactor Inlet Temperature (K) 550 540 700
Reactor Pressure 40 20 20
(Ethylene + CO + CO2) : Ethane Rates 1:1 1:1 1:1
Total Capital Investment (MM $) 92 81 74
Total Product Cost c/kg. 36.0 31.7 29.7
In the third column of table1, we give cost analysis after carrying out the following modifications;
1- The first two reactors are loaded with MoVNb catalyst and their reactants inlet temperature is above
650 K. At such a temperature the products are ethylene , carbon oxides and water with no acetic acid.
The gases are cooled to condense water.
2- The next two reactors are loaded with MoVNbPd catalyst. The gases from the first two reactors after
water removal are introduced at about 450-500 K. At this low temperature, ethylene is oxidized to
acetic acid with no water production. Water is however produced from the oxidation of ethylene to
 Moustafa Soliman et al. / APCBEE Procedia 3 (2012) 200 – 208 205

carbon oxides. Ethane is not oxidized. The acetic acid concentration could be then as high as 85%.
This saves cost of further concentrating the acid.
In table (2), we present the total capital cost calculations for the case of four fixed bed reactors. In table (3),
we present total product cost calculations. We notice from table (3) that oxygen contributes strongly to the
total product cost. This shows the importance of developing methods for cheaper oxygen production.

Table 2. Purchased equipment cost (MM $).

Equipment Purchased Cost

Reactors 2.4
Heat exchangers 2.8
Scrubber 0.4
Recycle compressor 1.5
Acetic acid concentration 4.4
Total 11.5

Fixed Capital Investment = Purchased Equipment Cost* Location factor (1.25)* Lang's Factor (4.8)
= 69 MM$
Total Capital Investment = Fixed Capital Investment/0.85= 81 MM$

Table 3. Production cost for acetic acid by ethane partial oxidation (136 Kt/year of acetic acid).

Raw Materials Quantity / kg. Price per Unit (c/kg) Unit Cost ( c )
Ethane 0.67 3.3 2.2
Oxygen 1.62 5.5 8.9
Catalyst 76*10-3 11000 1.7
Total Raw Materials 12.8
Power 0.1 Kwh 3 0.3
Cooling Water 0.01 m3. 30 0.3
Total Variable Cost 0.6
Total Direct Fixed Cost 13.4
(Labor, Maintenance, Plant Overhead, General Expenses,… 13.2
Depreciation 5.1
Total Product Cost 31.7

4. Discussion

The production of acetic acid by partial oxidation of ethane is a mature technology the economics of which
can be greatly improved, e.g., by further catalyst development, optimization of the operating conditions ,
better reactor design and energy integration . We notice that the production of one mole acetic acid and one
mole of ethylene are associated with the production of one mole of water. Thus, we get more concentrated
206 Moustafa Soliman et al. / APCBEE Procedia 3 (2012) 200 – 208

acid if we do not produce ethylene. This leads to savings in the acetic acid concentration section. Although
water vapor addition to the reactants improves acetic acid selectivity, its expensive separation from product
acetic acid makes this undesirable. In fact every effort should be made to reduce the amount of water. The
present paper presents a method for reducing tne amount of water associated with the acetic acid by oxidizing
ethane to ethylene first, then separating water produced followed by oxidation of ethylene to acetic acid.
Co-production of ethylene and acetic acid could be recommended if we could avoid the expensive
separation of ethylene from ethane. This can happen if the whole product is further processed to produce vinyl
acetate or ethyl acetate without the separation of ethane. The use of a fluidized bed followed by a fixed bed
reactor is an option that can be studied. The fluidized bed is designed such that not all oxygen is consumed
thus reducing catalyst volume. The oxygen remaining is further reacted in the fixed bed.Smejkal et al. [10]
obtained a product cost for acetic acid by carbonylation of methanol of 29c/kg.This can be increased to 34c/kg
due to the increase in equipment cost. Thus the partial oxidation process is very competitive with methanol
carbonylation. Our estimate and their estimate are very sensitive to the cost of raw materials. They used the
following prices 166$/t for methanol, and 50$/t for CO. In our case doubling the price of ethane increases
product cost by 2.2c/kg

5. Conclusions

From the study presented in this paper, we conclude that

1. The partial oxidation process is very competitive with methanol carbonylation.
2. Measures should be taken to reduce the amount of water associated with product acetic acid.
3. Cheaper methods for oxygen production need to be developed.
4. Catalyst research is important to improve catalyst performance and lifetime.
5. There is large scope for product cost reduction by process design optimization.

Acknowledgements

The authors acknowledge the support provided by King AbdulAziz City for Science and Technology for
the support of this research under grant number AR-29-256.

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